CN104944786B - A kind of low Jie's glass ceramics composite substrate material of low-temperature sintering and preparation method thereof - Google Patents
A kind of low Jie's glass ceramics composite substrate material of low-temperature sintering and preparation method thereof Download PDFInfo
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Abstract
The invention discloses low Jie's glass ceramics composite substrate material of a kind of low-temperature sintering and preparation method thereof, wherein, the low Jie's glass ceramics composite substrate material of low-temperature sintering is composed of the following components：The MKBS glass of 40wt%~62.5wt%, and 37.5wt%~60wt% Al2O3；The mol ratio of the MKBS glass is MgO：K2O：B2O3：SiO2=w：x：y：Z, wherein, 0.001<w<0.003,0.002<x<0.004,0.2<y<0.3,0.5<z<Al described in 0.62O3It is α types Al2O3.Formula of the invention is free of heavy metal component, can be applied in the product of high frequency field, green pollution-free；The preparation method of material of the present invention, less than 900 DEG C are dropped to for more than 1200 DEG C by traditional sintering process, and the further reduction of sintering temperature has power savings advantages；Excellent material property, dielectric constant is less than 5, and low (tan δ are lost<4×10‑3), temperature coefficient of resonance frequency stabilization, high mechanical strength (maximum is more than 110MPa).
Description
Technical field
It is multiple the invention belongs to medium glass ceramic composite substrate Material Field, more particularly to the low Jie's glass ceramics of low-temperature sintering
The method for closing baseplate material and its preparation.
Background technology
Developing rapidly for modern semiconductors industry, requirement higher is proposed to Electronic Packaging, and multi-layer substrate meets the tendency of
And give birth to.The application of low-temperature co-fired glass ceramic (LTCC) multilager base plate, improves the transmission speed and wiring density of signal, can be with
Meet the requirement of VLSI high-density packages, be the key foundation material of modern communication technology, defended in portable mobile phone, TV
Star receiver, military radar aspect have highly important application, miniaturization in modern communication instrument, it is integrated during just
Play increasing effect.The exploitation of low-temperature co-fired glass ceramic material system has turned into current Electronic Packaging area research
Focus.
The complication of component, densification and functionalization in electronic device and electronic installation, to package substrate and wiring work
Journey proposes higher and higher requirement, be mainly manifested in it is following some：(1) the high speed an urgent demand reduction dielectric of signal transmission is normal
Number, dielectric loss and reduction lead distance；(2) to reduce volume, many electronic components, such as resistance, even electric capacity, inductance will
It is built among substrate；(3) to reduce encapsulation volume, encapsulation link is reduced, bare chip actual load is the most typical.The many of encapsulation
Function, is such as electrically connected, physical protection, and stress relaxes, and radiating is moistureproof, dimensional transitions, normalization, standardization etc., just gradually portion
Divide or fully undertaken by substrate；(4) good chemical stability and mechanical performance.Traditional ceramics Al2O3Low dielectric in having
Constant (9~10), high mechanical properties (>400MPa), excellent chemical stability, is a kind of good baseplate material.However, pure
Al2O3Ceramic sintering temperature is (1400~1500 DEG C) higher, it is impossible to directly burnt altogether with the low-melting-point metal such as Ag, Cu.In order to reduce
Sintering temperature, it is incorporation low melting point oxide, such as B that traditional method is a kind of2O3And V2O5, but free B2O3And V2O5Rear
Slurry viscosity is easily caused in phase casting processes excessive and unstable, limits its practical application；Another method is Al2O3- crystallization
Glass, i.e., participate in a small amount of ceramics as nucleator in crystallized glass, and the final performance of product is decided by the crystallization degree of sample.
But the crystallized glass amount required for this method is very big, causes relatively costly, strongly limit glass ceramics composite substrate material
Development.
The content of the invention
Goal of the invention of the invention is：For above-mentioned problem, there is provided one kind can low-temperature sintering (850~900
DEG C), with low-k (﹤ 5), low-loss and frequency-temperature coefficient stabilization low Jie's glass ceramics composite substrate material and its
Preparation method.In can be applied to the civilian and national defense industry such as portable mobile phone, telstar receiver, military radar, work
Skill is simple, it is easy to industrialized production and strong mechanical property.
Technical solution of the invention is to provide a kind of low Jie's glass ceramics composite substrate material of low-temperature sintering and its system
Preparation Method, wherein, the low Jie's glass ceramics composite substrate material of low-temperature sintering is composed of the following components：40wt%~62.5wt%
MKBS glass, and 37.5wt%~60wt% Al2O3；The mol ratio of the MKBS glass is MgO：K2O：B2O3：
SiO2=w：x：y：Z, wherein, 0.001<w<0.003,0.002<x<0.004,0.2<y<0.3,0.5<z<0.6, the Al2O3For
α types Al2O3。
The preparation method of the low Jie's glass ceramics composite substrate material of low-temperature sintering as described above, comprises the following steps：
A, the component proportion according to the MKBS glass, by Mg (OH)2、K2CO3、SiO2And H3BO3Powder mixing；
, with deionized water as solvent, then wet ball-milling mixing dries for b, the mixed-powder that will be prepared in step a；
C, the powder after drying is melted in 1500 DEG C of air atmosphere high temperatures, MKBS glass fragments are formed after cooling；
D, by above-mentioned MKBS glass fragment with deionized water as solvent, wet ball-milling, then at 100 DEG C dry obtain
MKBS glass dust；
E, by above-mentioned MKBS glass dust with account for the Al that its percentage by weight is 60~150%2O3Mixing, be with deionized water
Solvent, wet ball-milling mixing, additive capacity accounts for the acrylic acid solution of the 2~5% of raw material gross mass and enters as binding agent after drying
Row granulation；
F, the particle for obtaining step e granulations are dry-pressing formed, and briquetting pressure is 10~20Mpa；
G, step f dry-pressing formed material is sintered in 850~900 DEG C of air atmospheres, be made low Jie's glass ceramics and answer
Close baseplate material.
Further, the wet ball-milling time in the step b and d be 5~10 hours, the wet ball-milling in step e
Time is 8~24 hours.
Further, the times after being dried in the step c in 1500 DEG C of air atmosphere high temperature meltings are 0.5~1 small
When, sintering time is 0.5~1 hour in 850~900 DEG C of air atmospheres in the step g.
Further, the type of cooling in the step c is water quenching.
Compared with prior art, beneficial effects of the present invention are embodied in：
1st, formula of the invention is free of heavy metal component, can be applied in the product of high frequency field, green pollution-free, full
The strict standard requirement of the RHOS and WEEE of the sufficient newest appearance of the European Community.
2nd, less than 900 DEG C are dropped to for more than 1200 DEG C by traditional sintering process, the further reduction of sintering temperature has energy-conservation
Advantage.
3rd, dielectric constant is less than 5, and low (tan δ are lost<4×10-3), temperature coefficient of resonance frequency stabilization, high mechanical strength
(maximum is more than 110MPa).
4th, the low Jie's glass ceramics composite substrate material of low-temperature sintering of the present invention can improve signal in the application of the communications field
Transmission speed and wiring density, can meet the requirement of VLSI high-density packages, be the key foundation material of modern communication technology,
There is highly important application in terms of portable mobile phone, telstar receiver, military radar, in modern communication instrument
Miniaturization, it is integrated during just playing increasing effect, with essential industry application value.
Brief description of the drawings
Fig. 1 is embodiment 3 in 850 degree of XRD (X-ray diffractogram) of sintering；
Fig. 2 is embodiment 5 in 850 degree of XRD (X-ray diffractogram) of sintering；
Fig. 3 is embodiment 7 in 850 degree of XRD (X-ray diffractogram) of sintering；
Fig. 4 is embodiment 3 in 850 degree of SEM (scanning electron microscope (SEM) photograph) of sintering；
Fig. 5 is embodiment 5 in 850 degree of SEM (scanning electron microscope (SEM) photograph) of sintering；
Fig. 6 is embodiment 7 in 850 degree of SEM (scanning electron microscope (SEM) photograph) of sintering.
Specific embodiment
Below in conjunction with drawings and Examples, the present invention is further illustrated.
A kind of low Jie's glass ceramics composite substrate material of low-temperature sintering, it is characterised in that composed of the following components：40wt%
The MKBS glass of~62.5wt%, and 37.5wt%~60wt% Al2O3；The mol ratio of the MKBS glass is MgO：
K2O：B2O3：SiO2=w：x：y：Z, wherein, 0.001<w<0.003,0.002<x<0.004,0.2<y<0.3,0.5<z<0.6, institute
State Al2O3It is α types Al2O3。
The preparation method of the low Jie's glass ceramics composite substrate material of low-temperature sintering as described above, comprises the following steps：
A, the component proportion according to the MKBS glass, by Mg (OH)2、K2CO3、SiO2And H3BO3Powder mixing；
, with deionized water as solvent, then wet ball-milling mixing dries for b, the mixed-powder that will be prepared in step a；
C, the powder after drying is melted in 1500 DEG C of air atmosphere high temperatures, MKBS glass fragments are formed after cooling；
D, by above-mentioned gained MKBS glass fragments with deionized water as solvent, then wet ball-milling is dried at 100 DEG C and is obtained
Obtain MKBS glass dust；
E, by above-mentioned MKBS glass dust with account for the Al that its percentage by weight is 60~150%2O3Mixing, be with deionized water
Solvent, wet ball-milling mixing, additive capacity accounts for the acrylic acid solution of the 2~5% of raw material gross mass and enters as binding agent after drying
Row granulation；
F, the particle for obtaining step e granulations are dry-pressing formed, and briquetting pressure is 10~20Mpa；
G, step f dry-pressing formed material is sintered in 850~900 DEG C of air atmospheres, be made low Jie's glass ceramics and answer
Close baseplate material.
Used as preferred, the wet ball-milling time in the step b and d is 5~10 hours, the wet type ball in step e
Consume time is 8~24 hours.
Used as preferred, the time after being dried in the step c in 1500 DEG C of air atmosphere high temperatures meltings is 0.5~1
Hour, sintering time is 0.5~1 hour in 850~900 DEG C of air atmospheres in the step g.
Preferably, the type of cooling in the step c is water quenching.
The low Jie's glass ceramics composite substrate material each component of embodiment of the present invention 1-8 low temperature sinterings is listed in table 1
Actual proportioning and sintering temperature.
The micro- of the low Jie's glass ceramics composite substrate material of low-temperature sintering obtained in 1-8 embodiments of the present invention is given in table 2
Ripple dielectric properties, the embodiment of the present invention carries out the evaluation of microwave dielectric property using cylindrical dielectric resonator method, and detection method is
GB/T7265.2-1987 open type cell method.
Table 1
Table 2
Embodiment 1
A, by Mg (OH)2、K2CO3、SiO2And H3BO3Powder mixing, its quality be respectively 0.0375g, 0.4175g,
26g and 21.05g；
B, by the above-mentioned powder for preparing with deionized water as solvent, wet ball-milling mix 6 hours, then dry；
C, the powder after drying is melted 1 hour in 1500 DEG C of air atmosphere high temperatures, MKBS glass is formed after cooling broken
Block；
D, by above-mentioned MKBS glass fragment with deionized water as solvent, wet ball-milling 6 hours, then at 100 DEG C dry
Obtain MKBS glass dust；
E, by above-mentioned MKBS glass dust and 52.5g Al2O3Mixing, with deionized water as solvent, wet ball-milling mixing 8 is small
When, additive capacity accounts for the acrylic acid solution of the 2~5% of raw material gross mass and is granulated as binding agent after drying；
F, the particle for obtaining above-mentioned granulation are dry-pressing formed, and briquetting pressure is 20Mpa；
G, step f dry-pressing formed material is sintered 1 hour in 850 DEG C of air atmospheres, be made low Jie's glass ceramics and answer
Close baseplate material.
Embodiment 2
A, by Mg (OH)2、K2CO3、SiO2And H3BO3Powder mixing, its quality is respectively 0.075g, 0.375g, 26g
And 21.05g；
, with deionized water as solvent, wet ball-milling mixes 6 hours, then dries for b, the powder for preparing step a；
C, the powder after drying is melted 1 hour in 1500 DEG C of air atmosphere high temperatures, MKBS glass is formed after cooling broken
Block；
D, by above-mentioned MKBS glass fragment with deionized water as solvent, wet ball-milling 6 hours, then at 100 DEG C dry
Obtain MKBS glass dust；
E, by above-mentioned MKBS glass dust and 52.5g Al2O3Mixing, with deionized water as solvent, wet ball-milling mixing 8 is small
When, additive capacity accounts for the acrylic acid solution of the 2~5% of raw material gross mass and is granulated as binding agent after drying；
F, the particle for obtaining above-mentioned granulation are dry-pressing formed, and briquetting pressure is 20Mpa；
G, step f dry-pressing formed material is sintered 1 hour in 875 DEG C of air atmospheres, be made low Jie's glass ceramics and answer
Close baseplate material.
Embodiment 3
A, by Mg (OH)2、K2CO3、SiO2And H3BO3Powder mixing, its quality is respectively 0.112g, 0.338g, 26g
And 21.05g；
, with deionized water as solvent, wet ball-milling mixes 6 hours, then dries for b, the powder for preparing step a；
C, the powder after drying is melted 1 hour in 1500 DEG C of air atmosphere high temperatures, MKBS glass is formed after cooling broken
Block；
D, by above-mentioned MKBS glass fragment with deionized water as solvent, wet ball-milling 6 hours, then at 100 DEG C dry
Obtain MKBS glass dust；
E, by above-mentioned MKBS glass dust and 52.5g Al2O3Mixing, with deionized water as solvent, wet ball-milling mixing 8 is small
When, additive capacity accounts for the acrylic acid solution of the 2~5% of raw material gross mass and is granulated as binding agent after drying；
F, the particle for obtaining above-mentioned granulation are dry-pressing formed, and briquetting pressure is 20Mpa；
G, step f dry-pressing formed material is sintered 1 hour in 850 DEG C of air atmospheres, be made low Jie's glass ceramics and answer
Close baseplate material.
Embodiment 4
A, by Mg (OH)2、K2CO3、SiO2And H3BO3Powder mixing, its quality be respectively 0.15g, 0.3g, 26g with
And 21.05g；
, with deionized water as solvent, wet ball-milling mixes 6 hours, then dries for b, the powder for preparing step a；
C, the powder after drying is melted 1 hour in 1500 DEG C of air atmosphere high temperatures, MKBS glass is formed after cooling broken
Block；
D, by above-mentioned MKBS glass fragment with deionized water as solvent, wet ball-milling 6 hours, then at 100 DEG C dry
Obtain MKBS glass dust；
E, by above-mentioned MKBS glass dust and 52.5g Al2O3Mixing, with deionized water as solvent, wet ball-milling mixing 8 is small
When, additive capacity accounts for the acrylic acid solution of the 2~5% of raw material gross mass and is granulated as binding agent after drying；
F, the particle for obtaining above-mentioned granulation are dry-pressing formed, and briquetting pressure is 20Mpa；
G, step f dry-pressing formed material is sintered 1 hour in 875 DEG C of air atmospheres, be made low Jie's glass ceramics and answer
Close baseplate material.
Embodiment 5
A, by Mg (OH)2、K2CO3、SiO2And H3BO3Powder mixing, its quality be respectively 0.15g, 0.3g, 26g with
And 21.05g；
, with deionized water as solvent, wet ball-milling mixes 6 hours, then dries for b, the powder for preparing step a；
C, the powder after drying is melted 1 hour in 1500 DEG C of air atmosphere high temperatures, MKBS glass is formed after cooling broken
Block；
D, by above-mentioned MKBS glass fragment with deionized water as solvent, wet ball-milling 6 hours, then at 100 DEG C dry
Obtain MKBS glass dust；
E, by above-mentioned MKBS glass dust and 52.5g Al2O3Mixing, with deionized water as solvent, wet ball-milling mixing 8 is small
When, additive capacity accounts for the acrylic acid solution of the 2~5% of raw material gross mass and is granulated as binding agent after drying；
F, the particle for obtaining above-mentioned granulation are dry-pressing formed, and briquetting pressure is 20Mpa；
G, step f dry-pressing formed material is sintered 1 hour in 850 DEG C of air atmospheres, be made low Jie's glass ceramics and answer
Close baseplate material.
Embodiment 6
A, by Mg (OH)2、K2CO3、SiO2And H3BO3Powder mixing, its quality is respectively 0.188g, 0.262g, 26g
And 21.05g；
, with deionized water as solvent, wet ball-milling mixes 6 hours, then dries for b, the powder for preparing step a；
C, the powder after drying is melted 1 hour in 1500 DEG C of air atmosphere high temperatures, MKBS glass is formed after cooling broken
Block；
D, by above-mentioned MKBS glass fragment with deionized water as solvent, wet ball-milling 6 hours, then at 100 DEG C dry
Obtain MKBS glass dust；
E, by above-mentioned MKBS glass dust and 52.5g Al2O3Mixing, with deionized water as solvent, wet ball-milling mixing 8 is small
When, additive capacity accounts for the acrylic acid solution of the 2~5% of raw material gross mass and is granulated as binding agent after drying；
F, the particle for obtaining above-mentioned granulation are dry-pressing formed, and briquetting pressure is 20Mpa；
G, step f dry-pressing formed material is sintered 1 hour in 875 DEG C of air atmospheres, be made low Jie's glass ceramics and answer
Close baseplate material.
Embodiment 7
A, by Mg (OH)2、K2CO3、SiO2And H3BO3Powder mixing, its quality is respectively 0.188g, 0.262g, 26g
And 21.05g；
, with deionized water as solvent, wet ball-milling mixes 6 hours, then dries for b, the powder for preparing step a；
C, the powder after drying is melted 1 hour in 1500 DEG C of air atmosphere high temperatures, MKBS glass is formed after cooling broken
Block；
D, by above-mentioned MKBS glass fragment with deionized water as solvent, wet ball-milling 6 hours, then at 100 DEG C dry
Obtain MKBS glass dust；
E, by above-mentioned MKBS glass dust and 52.5g Al2O3Mixing, with deionized water as solvent, wet ball-milling mixing 8 is small
When, additive capacity accounts for the acrylic acid solution of the 2~5% of raw material gross mass and is granulated as binding agent after drying；
F, the particle for obtaining above-mentioned granulation are dry-pressing formed, and briquetting pressure is 20Mpa；
G, step f dry-pressing formed material is sintered 1 hour in 850 DEG C of air atmospheres, be made low Jie's glass ceramics and answer
Close baseplate material.
Embodiment 8
A, by Mg (OH)2、K2CO3、SiO2And H3BO3Powder mixing, its quality is respectively 0.226g, 0.224g, 26g
And 21.05g；
, with deionized water as solvent, wet ball-milling mixes 6 hours, then dries for b, the powder for preparing step a；
C, the powder after drying is melted 1 hour in 1500 DEG C of air atmosphere high temperatures, MKBS glass is formed after cooling broken
Block；
D, by above-mentioned MKBS glass fragment with deionized water as solvent, wet ball-milling 6 hours, then at 100 DEG C dry
Obtain MKBS glass dust；
E, by above-mentioned MKBS glass dust and 52.5g Al2O3Mixing, with deionized water as solvent, wet ball-milling mixing 8 is small
When, additive capacity accounts for the acrylic acid solution of the 2~5% of raw material gross mass and is granulated as binding agent after drying；
F, the particle for obtaining above-mentioned granulation are dry-pressing formed, and briquetting pressure is 20Mpa；
G, step f dry-pressing formed material is sintered 1 hour in 875 DEG C of air atmospheres, be made low Jie's glass ceramics and answer
Close baseplate material.
The embodiment 1,4 and 8 being shown respectively by Fig. 1, Fig. 2 and Fig. 3 is in 850 degree of X-ray diffractograms of sintering, it is seen that with
Mg (OH)2Addition no third mutually generate, but structure is finer and close；The embodiment 1,4 that Fig. 4, Fig. 5 and Fig. 6 are shown respectively
With 8 in 850 degree of scanning electron microscope (SEM) photographs of sintering, it is seen then that Mg (OH) within the specific limits2Sintered density has been greatly facilitated, with reference to
The performance test results of table 2, the raising of sintered density further improves the dielectric properties and mechanical strength of glass ceramics.
One of ordinary skill in the art will be appreciated that embodiment described here is to aid in reader and understands this hair
Bright principle, it should be understood that protection scope of the present invention is not limited to such especially statement and embodiment.This area
Those of ordinary skill can according to these technical inspirations disclosed by the invention make it is various do not depart from essence of the invention other are each
Plant specific deformation and combine, these deformations and combination are still within the scope of the present invention.
Claims (5)
1. the low Jie's glass ceramics composite substrate material of a kind of low-temperature sintering, it is characterised in that composed of the following components：40wt%~
The MKBS glass of 62.5wt%, and 37.5wt%~60wt% Al2O3；The mol ratio of the MKBS glass is MgO：
K2O：B2O3：SiO2=w：x：y：Z, wherein, 0.001<w<0.003,0.002<x<0.004,0.2<y<0.3,0.5<z<0.6, institute
State Al2O3It is α types Al2O3。
2. the preparation method of the low Jie's glass ceramics composite substrate material of low-temperature sintering as claimed in claim 1, comprises the following steps：
A, the component proportion requirement according to the MKBS glass, by Mg (OH)2、K2CO3、SiO2And H3BO3Powder mixing；
B, by the above-mentioned mixed-powder for preparing with deionized water as solvent, wet ball-milling mixing, then dry；
C, the powder after above-mentioned drying is melted in 1500 DEG C of air atmosphere high temperatures, MKBS glass fragments are formed after cooling；
D, by above-mentioned MKBS glass fragment with deionized water as solvent, wet ball-milling, then at 100 DEG C dry, obtain MKBS
Glass dust；
E, by MKBS glass dust with account for the Al that its percentage by weight is 60~150%2O3Mixing, with deionized water as solvent, wet type
Ball milling mixing, additive capacity accounts for the acrylic acid solution of the 2~5% of raw material gross mass and is granulated as binding agent after drying；
F, the particle for obtaining above-mentioned granulation are dry-pressing formed, and briquetting pressure is 10~20Mpa；
G, above-mentioned dry-pressing formed material is sintered in 850~900 DEG C of air atmospheres, be made low Jie's glass ceramics composite base plate
Material.
3. the preparation method of the low Jie's glass ceramics composite substrate material of low-temperature sintering according to claim 2, its feature exists
In the wet ball-milling time in the step b and d is 5~10 hours, and the wet ball-milling time in step e is 8~24 small
When.
4. the preparation method of the low Jie's glass ceramics composite substrate material of low-temperature sintering according to Claims 2 or 3, its feature
It is that the time melted in 1500 DEG C of air atmosphere high temperatures after the drying in the step c is 0.5~1 hour, the step
Sintering time is 0.5~1 hour in 850~900 DEG C of air atmospheres in g.
5. the preparation method of the low Jie's glass ceramics composite substrate material of low-temperature sintering according to claim 2, its feature exists
In the cooling means of the step c is water quenching.
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